CN114350972A - Process for producing palladium sponge by using platinum-palladium concentrate chlorination leaching solution - Google Patents
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Abstract
The invention discloses a process for producing sponge palladium by utilizing platinum-palladium concentrate chlorination leaching solution, which comprises the following steps: s1, removing copper; s2, adjusting the PH value to be equal; s3, removing Si and Bi; s4, mixing the extracting agents to extract impurities; s5, removing oil by ultrasonic waves; s6, resin adsorption treatment; s7, repeatedly washing with hydrochloric acid; s8, acidifying the thiourea solution to desorb Pd; s9, reducing Pd; s10, heating and stirring in water bath at 40-50 ℃ for 2h, filtering, washing and drying in vacuum to obtain the sponge palladium product. The invention has the following advantages: 1. the method is suitable for the palladium-rich liquid with high impurities, and solves the problem that the high-impurity palladium-rich liquid is difficult to recover. 2. The invention has simple operation and can produce waste liquid with a loop. 3. The method for recovering the palladium in the platinum-palladium concentrate leaching solution has the advantages that the recovery rate can reach more than 92 percent, and the purity of the sponge palladium product is more than or equal to 99.95 percent.
Description
Technical Field
The invention relates to the field of rare and precious metal recovery production, in particular to a process for producing a palladium product by taking a platinum-palladium concentrate chlorination leaching solution as a raw material.
Background
The chloridizing leaching solution of the platinum-palladium concentrate is an intermediate product in the processing process flow of the copper anode mud, is rich in rare and precious metal elements such as palladium and the like, and is a main raw material for producing palladium products.
The noble metal palladium has special physical and chemical properties, is widely applied to aspects of national defense, science and technology, electronics, military industry and the like, and has very important function in national economy.
At present, the recovery preparation method of palladium products mainly comprises a chemical method and an extraction method. The chemical method mainly separates the precious metals of platinum and palladium from impurities in a form of precipitation, and has the defects of long flow path, large consumption of chemical reagents, large accumulation of precious metals and the like. The extraction method, which utilizes the difference in solubility of a solute in solvents that are not mutually soluble, is an operation for extracting a solute from a solution consisting of one solvent and another solvent, and is commonly used for extracting valuable metals from aqueous solutions. The method has the advantages of good metal selectivity, high recovery rate, renewable reagents, easy serialization and the like.
For example, the invention patent with publication number CN107058731A provides a method for preparing a palladium product by using platinum-palladium concentrate as a raw material, which comprises the following steps: controlling electrode potential oxidation leaching of platinum-palladium concentrate; performing ammonium chloride precipitation on the leaching solution to obtain a precipitated solution and a precipitation slag; mixing the precipitation slag and the precipitation liquid for slurrying, then carrying out reduction treatment, filtering to obtain filtrate and filter residue, and carrying out oxidation acid leaching on the filter residue to obtain a dissolved solution; the dissolved solution is subjected to S201 three-section countercurrent extraction to obtain palladium raffinate and palladium strip liquor; the palladium stripping solution is refined and reduced to obtain a palladium product. The method has strong adaptability of raw materials, simple operation and high product purity, but the process flow is relatively complicated, and multiple times of precipitation and impurity removal are needed, so that the production cost is high.
For example, patent of invention with publication number CN101713026A provides a method for extracting palladium from high-level radioactive waste liquid, which comprises: fully mixing the high-level radioactive waste liquid with a triisobutyl phosphine sulfide extracting agent; separating the palladium-containing extract phase after the extraction balance is achieved; washing the separated palladium-containing extract phase and repeating the steps for several times; adding a stripping agent into the washed palladium-containing extraction phase for stripping to obtain palladium stripping solution; the palladium stripping solution is refined and reduced to obtain a palladium product. The method has the advantages of good palladium selectivity, high back extraction rate and simple process equipment, but the triisobutyl phosphine sulfide mainly aims at the extraction of palladium in an HNO3 system, does not have universality and has higher requirements on the properties of raw materials.
Disclosure of Invention
The invention solves the technical problem that the process flow for producing palladium products in the prior art is long and cannot meet the requirement of industrial continuous production. Therefore, the method for producing sponge palladium in a short flow has the advantages of low cost, easy operation, high purity and continuous production.
The technical scheme adopted by the invention is as follows: a process for producing sponge palladium by utilizing platinum-palladium concentrate chlorination leaching liquid comprises the following steps: s1, adding oxalic acid into the chloridized leaching solution of the platinum-palladium concentrate, and filtering to obtain copper-removed solution and copper-removed slag; s2, adding sodium hydroxide to adjust the pH value of the copper-removed solution; s3, adding polyacrylamide for flocculation and sedimentation to remove part of Si and Bi, and filtering to obtain filtrate and filter residue; s4, adding a mixed extractant into the filtrate subjected to the S3 treatment to extract impurities, and removing gold; s5, ultrasonic degreasing is carried out on the gold extraction liquid treated by the S4, and the degreased liquid is obtained by adsorption and filtration of activated carbon; s6, adsorbing the deoiled liquid by using Puroite S920 resin to obtain palladium loaded resin and exchange tail liquid; s7, repeatedly washing the palladium-loaded resin by using hydrochloric acid, and washing out soluble metal impurities to obtain pure palladium-loaded resin and washing liquid; s8, desorbing Pd on the pure palladium-loaded resin by using an acidified thiourea solution to obtain a Pd desorption solution; s9, adding ascorbic acid into the Pd desorption solution to reduce Pd; s10, heating and stirring in water bath at 40-50 ℃ for 2h, filtering, washing and drying in vacuum to obtain the sponge palladium product.
As a further improvement of the invention, in step S2, the pH value of the solution after copper removal is controlled to be 1-2.
As a further improvement of the method, in the step S4, the mixed extracting agent is 1-3% of TBP and 97-99% of sec-octanol, and the extraction time is 10-15 minutes.
As a further improvement of the invention, in step S7, the hydrochloric acid is 0.3-1.0 mol/L hydrochloric acid.
As a further improvement of the invention, in step S9, the dosage of ascorbic acid is 2-3 times of the mass of palladium.
The invention has the following beneficial effects: compared with the prior art, the invention has the following advantages: 1. the method is suitable for the palladium-rich liquid with high impurities, and solves the problem that the high-impurity palladium-rich liquid is difficult to recover. 2. The invention has simple operation and can produce waste liquid with a loop. 3. The method for recovering the palladium in the platinum-palladium concentrate leaching solution has the advantages that the recovery rate can reach more than 92 percent, and the purity of the sponge palladium product is more than or equal to 99.95 percent.
Drawings
FIG. 1 is a schematic view of the process of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples.
A process for producing sponge palladium by utilizing platinum-palladium concentrate chlorination leaching liquid comprises the following steps:
s1, removing Cu in the platinum-palladium concentrate leachate in the form of copper oxalate precipitate by adding oxalic acid, reducing Pd (4+) into Pd (2+), and filtering to obtain a copper-removed solution and copper-removed slag; the Cu content in the platinum-palladium concentrate leachate is 1-2 g/L, and the Pd content is 2-3 g/;
s2, adding sodium hydroxide to adjust the pH value of the copper-removed solution, and controlling the pH value to be 1-2;
s3, adding a proper amount of polyacrylamide for flocculation and sedimentation to remove part of Si and Bi, and filtering to obtain filtrate and filter residue; the content of Si in the copper-removed liquid is 0.5-1 g/L, and the content of Bi is 0.4-0.7 g/L;
s4, adding a mixed extracting agent into the filtrate after the S3 treatment for impurity extraction, and removing gold contained in the filtrate; the content of Au in the filtrate is 0.2-0.5 g/L;
s5, ultrasonic degreasing is carried out on the gold extraction liquid treated by the S4, and the degreased liquid is obtained by adsorption and filtration of activated carbon; because the gold extraction liquid after extraction carries a small amount of grease more or less, the grease can be adsorbed on the surface of resin particles to cause the blockage of resin micropores, meanwhile, the grease can also cause the adhesion of the resin to cause unsmooth or uneven water flow of a resin layer to generate bias flow, and the effect of ion exchange can be reduced. Therefore, the problems can be solved by using ultrasonic wave to remove oil, and the effect of adsorbing palladium by the ion exchange resin is improved.
S6, adsorbing the deoiled liquid by using Puroite S920 resin to obtain palladium loaded resin and exchange tail liquid; puroite S920 resin is a resin brand called bleaching company in Chinese, and S920 is a special resin model and mainly used for adsorbing platinum group noble metals.
S7, repeatedly washing the palladium-loaded resin by using hydrochloric acid, and washing out soluble metal impurities to obtain pure palladium-loaded resin and washing liquid;
s8, desorbing Pd on the pure palladium-loaded resin by using an acidified thiourea solution to obtain a Pd desorption solution;
s9, adding ascorbic acid into the Pd desorption solution to reduce Pd;
s10, heating and stirring in water bath at 40-50 ℃ for 2h, filtering, washing and drying in vacuum to obtain the sponge palladium product.
The invention firstly uses oxalic acid to mainly reduce Pd (4+) in a solution to Pd (2+), ion exchange resin mainly adsorbs Pd (2+), and the step mainly provides a cushion for the subsequent ion exchange step; meanwhile, the oxalic acid can form copper oxalate precipitates with Cu ions in the solution to achieve the effect of copper removal, and the influence of Cu on the subsequent TBP extraction can be reduced as much as possible. Compared with the traditional oxalic acid which is only used as a back extractant, the two effects are different.
Example 1:
firstly, taking 1L of platinum-palladium concentrate leachate, adding 90g of oxalic acid into the leachate, stirring for 1h in water bath at 80 ℃, standing for 12h, and filtering to obtain copper-removed solution and copper-removed slag; then, adding 20g of sodium hydroxide into the copper-removed solution to control the pH value to be 1, adding 0.2g of polyacrylamide to perform flocculation and sedimentation to remove partial impurities such as Si, Bi and the like, and filtering to obtain filtrate and filter residue; extracting the filtrate by using a TBP (1%) + secondary octanol (99%) mixed extracting agent for 10min according to the O/A (1), performing secondary extraction, and removing gold contained in the filtrate by impurity extraction, wherein the impurity extraction rate of gold is more than or equal to 99%; degreasing the gold-extracted solution by ultrasonic waves for 0.5h, and adsorbing and filtering by activated carbon to obtain degreased solution; repeatedly treating the deoiled solution for 3-4 times by using Puroite S920 resin to obtain palladium loaded resin and exchange tail solution, wherein the total adsorption rate of palladium is more than or equal to 96%; repeatedly washing the palladium-loaded resin for 2-3 times by using 0.5mol/L hydrochloric acid, and washing away most soluble metal impurities to obtain pure palladium-loaded resin; repeatedly desorbing the pure palladium-loaded resin for 2-3 times by using a thiourea solution with hydrochloric acid acidification concentration of 10% to obtain a Pd desorption solution, wherein the desorption rate of palladium is more than or equal to 97%; and adding 6g of ascorbic acid into the Pd desorption solution to reduce Pd, heating and stirring in a water bath at 40-50 ℃ for 2 hours, filtering, washing and drying in vacuum to obtain a sponge palladium product.
Example 2:
firstly, taking 1L of platinum-palladium concentrate leachate, adding 100g of oxalic acid into the leachate, stirring for 1h in water bath at 85 ℃, standing for one night, and filtering to obtain copper-removed solution and copper-removed slag; secondly, adding 20g of sodium hydroxide into the copper-removed solution to control the pH value to be 1-2, adding 0.1g of polyacrylamide to perform flocculation and sedimentation to remove partial impurities such as Si, Bi and the like, and filtering to obtain filtrate and filter residue; extracting the filtrate by using a TBP (1.5%) + secondary octanol (98.5%) mixed extracting agent for 10min according to the O/A (1), performing secondary extraction, and removing gold contained in the filtrate by impurity extraction, wherein the impurity extraction rate of gold is more than or equal to 99%; degreasing the gold-extracted solution for 1h by using ultrasonic waves, and adsorbing and filtering by using activated carbon to obtain degreased solution; repeatedly treating the deoiled solution for 3-4 times by using Puroite S920 resin to obtain palladium loaded resin and exchange tail solution, wherein the total adsorption rate of palladium is more than or equal to 96%; repeatedly washing the palladium-loaded resin for 2-3 times by using 1mol/L hydrochloric acid, and washing away most soluble metal impurities to obtain pure palladium-loaded resin; repeatedly desorbing the palladium-loaded resin for 2-3 times by using a thiourea solution with hydrochloric acid acidification concentration of 10% to obtain a Pd desorption solution, wherein the desorption rate of palladium is more than or equal to 97%; adding 8g of ascorbic acid into the Pd desorption solution to reduce Pd, heating and stirring in a water bath at 40-50 ℃ for 2h, filtering, washing and drying in vacuum to obtain a sponge palladium product.
Example 3:
firstly, taking 1L of platinum-palladium concentrate leachate, adding 110g of oxalic acid into the leachate, stirring for 1h in a water bath at 90 ℃, standing for one night, and filtering to obtain copper-removed solution and copper-removed slag; then, adding 20g of sodium hydroxide into the copper-removed solution to control the pH value of the copper-removed solution to be 1-2, adding 0.2g of polyacrylamide to perform flocculation and sedimentation to remove partial impurities such as Si, Bi and the like, and filtering to obtain filtrate and filter residue; extracting the filtrate with TBP (2%) + secondary octanol (98%) for 15min in a secondary extraction process with O/A of 0.5, wherein the gold content in the filtrate can be removed, and the gold extraction rate is not lower than 99%; removing oil from the gold-extracted solution by ultrasonic waves for 1h, and adsorbing and filtering by activated carbon to obtain oil-removed solution; repeatedly treating the deoiled solution for 3-4 times in the fourth step by using Puroite S920 resin to obtain palladium loaded resin and exchange tail solution, wherein the total adsorption rate of palladium is more than or equal to 96%; repeatedly washing the palladium-loaded resin for 2-3 times by using 1mol/L hydrochloric acid, and washing away most soluble metal impurities to obtain pure palladium-loaded resin; repeatedly desorbing the palladium-loaded resin for 2-3 times by using a thiourea solution with hydrochloric acid acidification concentration of 15% to obtain a Pd desorption solution, wherein the desorption rate of palladium is more than or equal to 98%; adding 10g of ascorbic acid into the Pd desorption solution to reduce Pd, heating and stirring in a water bath at 40-50 ℃ for 2h, filtering, washing and drying in vacuum to obtain a sponge palladium product.
Finally, the results of the tests on the sponge palladium products of examples 1 to 3 are given, and the chemical compositions are shown in the following table (unit: ppm).
| Detecting element | Example 1 | Example 2 | Example 3 |
| Pd | 99.977％ | 99.980％ | 99.969％ |
| Pt | 160 | 135 | 190 |
| Si | 13 | 17 | 30 |
| Al | 2.8 | 3 | 5 |
| Bi | 0.52 | 0.64 | 0.34 |
| Cr | 0.35 | 0.21 | 0.89 |
| Cu | 0.59 | 0.45 | 0.78 |
| Fe | 5.43 | 3.26 | 2.98 |
| Ir | 0.1 | 0.1 | 0.1 |
| Mg | 2.17 | 1.78 | 4.57 |
| Mn | 0.29 | 0.15 | 0.32 |
| Ni | 0.43 | 0.8 | 1.1 |
| Pb | 2.94 | 3.17 | 5.67 |
| Rh | 0.28 | 0.15 | 0.2 |
| Ru | 0.1 | 0.1 | 0.1 |
| Sn | 0.1 | 0.1 | 0.1 |
| Zn | 15.5 | 17.88 | 20.7 |
| Ag | 17.91 | 12.4 | 30.2 |
| Au | 6.42 | 5.24 | 14.3 |
According to the detection, the purity of the sponge palladium is high and can reach the standard of SM-Pd 99.95, impurities in the sponge palladium are well removed, and more importantly, the process is short in flow and can achieve efficient recovery of palladium.
It should be understood by those skilled in the art that the protection scheme of the present invention is not limited to the above-mentioned embodiments, and various permutations, combinations and modifications can be made on the above-mentioned embodiments without departing from the spirit of the present invention, and the modifications are within the scope of the present invention.
Claims (5)
1. A process for producing sponge palladium by utilizing platinum-palladium concentrate chlorination leaching liquid comprises the following steps:
s1, adding oxalic acid into the chloridized leaching solution of the platinum-palladium concentrate, and filtering to obtain copper-removed solution and copper-removed slag;
s2, adding sodium hydroxide to adjust the pH value of the copper-removed solution;
s3, adding polyacrylamide for flocculation and sedimentation to remove part of Si and Bi, and filtering to obtain filtrate and filter residue;
s4, adding a mixed extractant into the filtrate subjected to the S3 treatment to extract impurities, and removing gold;
s5, ultrasonic degreasing is carried out on the gold extraction liquid treated by the S4, and the degreased liquid is obtained by adsorption and filtration of activated carbon;
s6, adsorbing the deoiled liquid by using Puroite S920 resin to obtain palladium loaded resin and exchange tail liquid;
s7, repeatedly washing the palladium-loaded resin by using hydrochloric acid, and washing out soluble metal impurities to obtain pure palladium-loaded resin and washing liquid;
s8, desorbing Pd on the pure palladium-loaded resin by using an acidified thiourea solution to obtain a Pd desorption solution;
s9, adding ascorbic acid into the Pd desorption solution to reduce Pd;
s10, heating and stirring in water bath at 40-50 ℃ for 2h, filtering, washing and drying in vacuum to obtain the sponge palladium product.
2. The process of claim 1, wherein in step S2, the pH of the copper-removed solution is controlled to be 1-2.
3. The process of claim 1, wherein in step S4, the mixed extractant comprises 1-3% TBP and 97-99% sec-octanol, and the extraction time is 10-15 minutes.
4. The process of claim 1, wherein the hydrochloric acid in step S7 is 0.3-1.0 mol/L hydrochloric acid.
5. The process for producing palladium sponge by using the chloridizing leaching solution of platinum-palladium concentrate according to any one of claims 1 to 4, wherein the using amount of the ascorbic acid in the step S9 is 2-3 times of the mass of the palladium.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117049971A (en) * | 2023-08-22 | 2023-11-14 | 株洲环冠新材料科技有限公司 | Amino modified material and preparation method and application thereof |
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